CN102174711B - Method using high thermal stability film as MTG (melt textured growth) seed crystal to prepare high temperature superconducting material - Google Patents
Method using high thermal stability film as MTG (melt textured growth) seed crystal to prepare high temperature superconducting material Download PDFInfo
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- CN102174711B CN102174711B CN2011100608668A CN201110060866A CN102174711B CN 102174711 B CN102174711 B CN 102174711B CN 2011100608668 A CN2011100608668 A CN 2011100608668A CN 201110060866 A CN201110060866 A CN 201110060866A CN 102174711 B CN102174711 B CN 102174711B
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Abstract
The invention relates to a method using a high thermal stability film as MTG (melt textured growth) seed crystal to prepare a high temperature superconducting material, and the method belongs to the technical field of high temperature superconducting materials. A 123-phase rare-earth element and a 211-phase rare-earth element are mixed with silver element according to the molar percentages of (50-60):(25-40):(1-15), the mixture is subjected to the preliminary grinding and roasting treatment, and a rough blank of a superconducting material can be obtained and then is subjected to preforming treatment, and roasted and cooled to obtain the seed crystal for the high temperature superconducting material. In the method, a low melting point YBCO/LAO seed film is utilized to texture and grow a single domain REBCO bulk, and is significant to research and development of the bulk having wide application prospect.
Description
Technical field
What the present invention relates to is a kind of method of high temperature superconducting materia technical field, specifically is a kind of high thermal stability film YBa
2Cu
3Ox/LaAlO
3(YBCO/LAO) seed crystal as the melting texture method prepares high temperature superconducting materia.
Background technology
Owing to have superconducting transition temperature and the application prospects that is higher than liquid nitrogen temperature, the REBCO material is the emphasis of people's research in the high-temperature superconductor field always.In numerous technologies of preparing, melting texture method (Melt Textured Growth is called for short MTG) is to control spontaneous nucleation and oriented growth through adding seed crystal, makes a kind of growth method of high-temperature superconductor block material textureization.In the REBCO block materials that this method is prepared, RE
2Ba
1Cu
1Ox (RE211) particle can become pinning center, thereby obtains high critical current density, helps the realization of large size high-performance high temperature superconducting materia, is a kind of technology of preparing that has much market potential.
In the preparation method of this high temperature superconducting materia of melting texture growing, selecting suitable kind film or seed crystal all is the key of triturating.Aspect film preparation, the YBCO oxide superconductor is simple in structure at present, and it is single-phase to obtain superconduction easily, has advantages such as preparation technology is simple, good reproducibility, and is the most ripe in the REBCO thin film preparation process, is the splendid selection as seed crystal.
Retrieval through to prior art is found; " The phenomenon of the superheating of YBCO thin film andits application in processing REBCO bulk " (thermal behavior excessively of YBCO/MgO film and application in the preparation of REBCO block materials; Supercond.Sci.Technol.19; (2006); S423-S428.) put down in writing the fusing not yet under the temperature that is higher than its fusing point 50K of a kind of YBCO/MgO film in, and gone out to be higher than the REBCO bulk of YBCO Peritectic Reaction temperature with melting texture method success extension.But the area that should technology texture goes out the REBCO bulk is very undesirable, and single domain REBCO block materials still is difficult to prepare successfully.This needs a kind of kind film with high thermal stability more as seed crystal.
Summary of the invention
The present invention is directed to the above-mentioned deficiency that prior art exists; Provide a kind of high thermal stability film to prepare high-temperature superconductor block material as the seed crystal of melting texture method; Be deposited in the melting process of the ybco film on the monocrystalline lanthanum aluminate substrate in Real Time Observation; Discovery is higher than more than the ybco film 30K that is deposited on the Natural manganese dioxide being higher than the thawing fully yet of the above ybco film of its Peritectic Reaction temperature (Tp) 80K.Utilize the high heat stability character of this film, can be used as the seed crystal of melting texture growing, be used to prepare dystectic single domain REBCO superconducting material.
The present invention realizes through following technical scheme:
The present invention relates to the method that a kind of seed crystal prepares high-temperature superconductor block material; Through 123 phase REEs are mixed after REE and the silver element molar percentage batching according to 50-60: 25-40: 1-15 with 211 mutually; After preliminary grinding calcination processing, obtain the superconducting material crude green body, obtain high-temperature superconductor block material after calcination and the cooling carrying out behind the superconducting material crude green body compressing tablet.
Described 123 phase REEs with 211 mutually REE be meant: Gd123 and Gd211, Nd123 and Nd211 or Sm123 and Sm211.
Described preliminary grinding calcination processing is meant: mixed former abrasive lapping is placed under 890-910 ℃ the environment and carries out the calcining more than 40-50 hour, the calcining back that finishes is repeated above-mentioned steps and is carried out regrind and secondary clacining, obtains the superconducting material crude green body;
Described compressing tablet is meant: the superconducting material crude green body is pressed into circular pie structure.
Described calcination is meant: add the ybco film that is deposited on the monocrystalline lanthanum aluminate through the top of the superconducting material crude green body behind the compressing tablet as seed crystal; Place reactors then; In 4-6 hour, be warming up to 1090-1100 ℃ and be incubated 2-3 hour; Fast cooling is to 1015-1055 ℃ and be incubated 40-80 hour, quenches to make block materials.
The present invention relates to the seed crystal that method for preparing obtains and prepare high-temperature superconductor block material, below liquid nitrogen temperature, have superconductivity, have the superconducting transition temperature Tc of 89-95K.
The inventive method adopts the YBCO/LAO film with high thermal stability as the seed crystal in the melting texture growing.This novel seed crystal has and is prone to preparation, high quality, be prone to cutting, than characteristics such as the YBCO/MgO film heat stability are higher.Be difficult to prepare under the situation with dystectic high quality REBCO film, going out single domain REBCO block materials with lower melting point YBCO/LAO kind film texture growing.Development to block materials is significant.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1:YBCO/LAO film as seed crystal melting texture growing GdBCO superconduction bulk material
1, prepares burden according to the Gd123+30mol%Gd211+10mol%Ag component;
2, grind, 910 ℃ of insulations were calcined in 48 hours, ground again, adopted the same process secondary clacining;
3, be pressed into
circular pie structure; The top adds the YBCO/LAO film as seed crystal of 2mm*2mm, and this whole system is put into reactors;
4, be warming up to 1090 ℃ in 4 hours, be incubated 2 hours, fast cooling to 1015 ℃ is incubated 80 hours, and quenching obtains single domain GdBCO block materials.
The physicochemical characteristic of the high-temperature superconductor block material that present embodiment prepares is: be of a size of
and below liquid nitrogen temperature, have superconductivity, have the superconducting transition temperature (Tc) about 91K.
Embodiment 2:YBCO/LAO film as seed crystal melting texture growing NdBCO superconduction bulk material
1, prepares burden according to the Nd123+25mol%Nd211+15mol%Ag component;
2, grind, 900 ℃ of insulations were calcined in 50 hours, ground again, adopted the same process secondary clacining;
3, be pressed into
circular pie structure; The top adds the YBCO/LAO film as seed crystal of 2mm*2mm, and this whole system is put into reactors;
4, be warming up to 1100 ℃ in 5 hours, be incubated 3 hours, fast cooling to 1055 ℃ is incubated 60 hours, and quenching obtains single domain NdBCO block materials.
The physicochemical characteristic of the high-temperature superconductor block material that present embodiment prepares is: be of a size of
and below liquid nitrogen temperature, have superconductivity, have the superconducting transition temperature (Tc) about 93K.
Embodiment 3:YBCO/LAO film as seed crystal melting texture growing SmBCO superconduction bulk material
1, prepares burden according to the Sm123+35mol%Sm211+15mol%Ag component;
2, grind, 890 ℃ of insulations were calcined in 50 hours, ground again, adopted the same process secondary clacining;
3, be pressed into
circular pie structure; The top adds the YBCO/LAO film as seed crystal of 2mm*2mm, and this whole system is put into reactors;
4, be warming up to 1095 ℃ in 4 hours, be incubated 2.5 hours, fast cooling to 1035 ℃ is incubated 70 hours, and quenching obtains single domain SmBCO block materials.
The physicochemical characteristic of the high-temperature superconductor block material that present embodiment prepares is: be of a size of
and below liquid nitrogen temperature, have superconductivity, have the superconducting transition temperature (Tc) about 92K.
Claims (6)
1. a seed crystal prepares the method for high-temperature superconductor block material; It is characterized in that; Use the ybco film that is deposited on the monocrystalline lanthanum aluminate as seed crystal; Through with 123 phase REEs with 211 mutually REE and silver element mixes according to the molar percentage batching back of 50-60:25-40:1-15, after preliminary grinding calcination processing, obtain the superconducting material crude green body, obtain high-temperature superconductor block material with carrying out behind the superconducting material crude green body compressing tablet after calcination is also cooled off.
2. seed crystal according to claim 1 prepares the method for high-temperature superconductor block material, it is characterized in that, described 123 phase REEs with 211 mutually REE be meant: Gdl23 and Gd211, Nd123 and Nd211 or Sm123 and Sm211.
3. seed crystal according to claim 1 prepares the method for high-temperature superconductor block material; It is characterized in that; Described preliminary grinding calcination processing is meant: mixed former abrasive lapping is placed under 890-910 ℃ the environment and carries out the calcining more than 40-50 hour; Repeat above-mentioned steps after calcining finishes and carry out regrind and secondary clacining, obtain the superconducting material crude green body.
4. seed crystal according to claim 1 prepares the method for high-temperature superconductor block material, it is characterized in that, described compressing tablet is meant: the superconducting material crude green body is pressed into circular pie structure.
5. a high-temperature superconductor block material is characterized in that, prepares according to each described method among the claim 1-4.
6. high-temperature superconductor block material according to claim 5 is characterized in that this material has the superconducting transition temperature Tc of 89-95K.
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| CN103172361A (en) * | 2011-12-20 | 2013-06-26 | 北京有色金属研究总院 | Process for avoiding seed crystal melting in preparation of silver-doped high temperature superconductive bulks through melt texture method |
| CN102586876B (en) * | 2012-02-08 | 2015-07-15 | 上海交通大学 | Preparation method of Russian export blend crude oil (REBCO) high-temperature superconducting block materials |
| CN102877124B (en) * | 2012-09-20 | 2015-06-17 | 上海交通大学 | Method for preparing wide-crack spacing REBCO high-temperature superconducting thick films using YBCO/LAO seed films |
| CN104178808B (en) * | 2014-08-06 | 2017-01-25 | 上海交通大学 | Liquid-phase epitaxial method for preparing high-temperature superconductive artificial crystal boundary |
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|---|---|---|---|---|
| CN1970848A (en) * | 2006-11-02 | 2007-05-30 | 上海交通大学 | Process for homo-epitaxial growth of superconductive block materials with rare earth Ba-Cu-O film as seed crystal |
| CN101279847A (en) * | 2008-05-29 | 2008-10-08 | 上海交通大学 | Preparation for YBCO Superconducting bulk doped with trace rare-earth element |
| CN101319379A (en) * | 2008-05-15 | 2008-12-10 | 上海交通大学 | Method for 45 degree rare earth barium copper oxygen thin film seed high speed growth superconducting block material |
| CN101717256A (en) * | 2009-12-21 | 2010-06-02 | 上海交通大学 | Method for preparing rare earth barium copper oxide superconducting block material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970848A (en) * | 2006-11-02 | 2007-05-30 | 上海交通大学 | Process for homo-epitaxial growth of superconductive block materials with rare earth Ba-Cu-O film as seed crystal |
| CN101319379A (en) * | 2008-05-15 | 2008-12-10 | 上海交通大学 | Method for 45 degree rare earth barium copper oxygen thin film seed high speed growth superconducting block material |
| CN101279847A (en) * | 2008-05-29 | 2008-10-08 | 上海交通大学 | Preparation for YBCO Superconducting bulk doped with trace rare-earth element |
| CN101717256A (en) * | 2009-12-21 | 2010-06-02 | 上海交通大学 | Method for preparing rare earth barium copper oxide superconducting block material |
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